WO2022100647A1 - Matériau polymère fluorescent vert, son procédé de préparation et son utilisation - Google Patents

Matériau polymère fluorescent vert, son procédé de préparation et son utilisation Download PDF

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WO2022100647A1
WO2022100647A1 PCT/CN2021/130000 CN2021130000W WO2022100647A1 WO 2022100647 A1 WO2022100647 A1 WO 2022100647A1 CN 2021130000 W CN2021130000 W CN 2021130000W WO 2022100647 A1 WO2022100647 A1 WO 2022100647A1
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Prior art keywords
ceramic material
green fluorescent
graphene
fluorescent ceramic
green
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PCT/CN2021/130000
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English (en)
Chinese (zh)
Inventor
周有福
洪茂椿
凌军荣
张修强
李春松
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中国科学院福建物质结构研究所
福建中科芯源光电科技有限公司
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Priority to US18/252,400 priority Critical patent/US20240002722A1/en
Publication of WO2022100647A1 publication Critical patent/WO2022100647A1/fr

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    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C04B2235/9646—Optical properties
    • C04B2235/9653—Translucent or transparent ceramics other than alumina
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C04B2235/9646—Optical properties
    • C04B2235/9661—Colour

Definitions

  • the invention belongs to the field of transparent fluorescent materials for LEDs, and in particular relates to a green fluorescent ceramic material and a preparation method and application thereof.
  • LED has excellent properties such as high luminous efficiency, energy saving and environmental protection, and long life, and is widely used in outdoor lighting, stadium lighting, indoor lighting and other fields.
  • the traditional LED light source is to encapsulate Y 3 Al 5 O 12 :Ce (YAG:Ce) phosphors in epoxy resin or silica gel.
  • These organic packaging materials have poor heat dissipation, and the heat is not easily dissipated during the working process of the LED chip, resulting in a rise in the temperature of the light source. Long-term work results in the aging and decomposition of organic packaging materials, resulting in problems such as light decay, color shift and reduced working life.
  • YAG:Ce fluorescent transparent ceramics have higher thermal conductivity and thermal stability, and are used as LED packaging materials to effectively solve the problems of light decay, color shift, and life reduction caused by poor heat dissipation of organic packaging materials.
  • YAG:Ce fluorescent ceramics are used as light conversion materials, the LEDs encapsulated by YAG:Ce phosphors and the LEDs encapsulated by YAG:Ce phosphors are both white LEDs, which cannot meet the lighting needs of special occasions.
  • green LEDs include: 1) For deep-sea fishing, compared with metal halide/traditional packaged LED green fish light, it has higher luminous efficiency and better heat dissipation; 2) Green LED matching The red fluorescent material can realize full-spectrum lighting, improve color rendering and luminous quality; 3) Green LEDs have broad application prospects in the fields of underwater visible light communication technology, vegetable cultivation, and poultry egg hatching.
  • high-end lighting market such as high-power LED special lighting is in the ascendant, and higher requirements are placed on the luminous band and heat dissipation of fluorescent ceramics. packaging requirements.
  • Lu 3 Al 5 O 12 :Ce(LuAG:Ce) is a green transparent ceramic with excellent performance, which can not only be excited by blue light effectively, but also has excellent thermal stability.
  • literature reports Xu, J., et al., Journal of the European Ceramic Society, 38(1), 343-347
  • the luminous intensity of LEDs encapsulated by LuAG:Ce fluorescent ceramics decreased by only 4.1% at 220 °C ; After 1000h of continuous operation, the luminous intensity decreased by only 1.9%.
  • patent document CN201510234002.1 discloses a kind of LuAG:Ce green fluorescent ceramics, Lutetium Lu is expensive, and the production cost of LuAG:Ce ceramics is relatively high, which greatly limits its application range.
  • Graphene is an excellent two-dimensional material with high transmittance and high thermal conductivity (3500Wm -1 K -1 ).
  • Many studies have shown that the introduction of graphene into TiC, Al 2 O 3 , AlN, SiO 2 , Si 3 N 4 , SiC and other ceramic substrates has achieved remarkable results in terms of mechanical properties, thermal properties, and electrical properties.
  • introducing 2wt% graphene into the SiC matrix can increase the thermal conductivity from 114Wm -1 K -1 to 145Wm -1 K -1 .
  • the introduction of graphene will hinder the sintering and densification of the ceramic matrix, so hot pressing sintering, spark plasma sintering, high frequency induction heating sintering and other sintering methods with high equipment requirements are usually used to prepare graphene-ceramic composites.
  • the vacuum sintering method is easier to prepare large-sized and complex-shaped ceramic products than the above-mentioned methods, and at the same time provides additional driving force to eliminate pores and promote the densification of products.
  • YAG:Ce/LuAG:Ce fluorescent ceramics prepared by vacuum sintering method need to be annealed in air to eliminate oxygen vacancy defects, and graphene is easy to oxidize and decompose when annealed in air, so graphene modified densified fluorescent ceramics are prepared by vacuum sintering method Composite materials are extremely challenging work.
  • the invention provides a green fluorescent ceramic material, the chemical composition of which is graphene-Y 3-xy Al 5 O 12 :xCe 3+ , yLu 3+ , wherein 0.0001 ⁇ x ⁇ 0.1, 0.01 ⁇ y ⁇ 2.9; Based on the total weight of the green fluorescent ceramic material, the mass percentage of the graphene is less than 0.5 wt % but not 0.
  • the value range of x is 0.0005 ⁇ x ⁇ 0.06, preferably 0.001 ⁇ x ⁇ 0.01; 0.04, 0.05, 0.06, 0.07, 0.08, 0.09, 0.1.
  • the value range of y is 0.1 ⁇ y ⁇ 2.5, preferably 0.5 ⁇ y ⁇ 1.5, and exemplarily 0.01, 0.05, 0.1, 0.5, 1, 1.5, 2.5, 2.9.
  • the mass fraction of the graphene is less than or equal to 0.1 wt % and not 0; preferably, the mass fraction of the graphene is less than or equal to 0.05 wt % % and not 0; Exemplary 0.001wt%, 0.002wt%, 0.004wt%, 0.005wt%, 0.006wt%, 0.008wt%, 0.01wt%, 0.015wt%, 0.02wt%, 0.025wt%, 0.03 wt %, 0.035 wt %, 0.04 wt %, 0.045 wt %, 0.05 wt %, 0.1 wt %, 0.2 wt %, 0.3 wt %, 0.4 wt %, or 0.45 wt %.
  • the chemical composition of the green fluorescent ceramic material is:
  • the green fluorescent ceramic material is a transparent ceramic material.
  • the visible light transmittance of the green fluorescent ceramic material is greater than or equal to 75%, preferably greater than or equal to 78%, exemplarily 75%, 76%, 78%, 79%, 80%, 81% or 82%.
  • the thermal conductivity of the green fluorescent ceramic material is greater than 5Wm -1 K -1 ; preferably greater than or equal to 7Wm -1 K -1 ; also preferably greater than or equal to 10Wm -1 K -1 ; exemplarily 7.0 Wm - 1K - 1 , 7.2Wm - 1K- 1 , 10.0Wm-1K- 1 , 11.2Wm-1K - 1 , 12.1Wm-1K - 1 , 13.2Wm-1K - 1 .
  • the present invention also provides a preparation method of the green fluorescent ceramic material, the preparation method comprising the following steps:
  • the green fluorescent ceramic material is prepared by vacuum sintering the ceramic green body obtained in the powder embedding step 2).
  • the sintering aid is one, two or more of CaO, MgO, SiO 2 and TEOS, preferably a combination of CaO and TEOS, MgO, or a combination of MgO and TEOS.
  • the Ce-containing compound may be selected from CeO 2 and/or CeN 3 O 9 ⁇ 6H 2 O.
  • the mass fraction of CaO or MgO is 0.001-0.01wt%, for example, 0.003-0.008 wt %, exemplarily 0.001 wt %, 0.002 wt %, 0.003 wt %, 0.004 wt %, 0.006 wt %, 0.008 wt %, 0.01 wt %.
  • the mass fraction of SiO 2 or TEOS is 0.01-0.1 wt %, for example, 0.03 - 0.08 wt%, exemplarily 0.01 wt%, 0.02 wt%, 0.03 wt%, 0.04 wt%, 0.06 wt%, 0.08 wt%, 0.1 wt%.
  • the ball milling is a wet ball milling.
  • the medium of the ball milling is absolute ethanol or acetone.
  • the time of the ball milling is 4h-30h, preferably 8h-24h.
  • the preparation of the ceramic green body in step 2) is specifically: the slurry obtained in step 1) is dried, sieved, dry pressed, cold isostatic pressing, and debonded to obtain the ceramic green body. .
  • the drying is vacuum drying, for example, the drying temperature is 50-70°C, preferably 55-65°C, and exemplarily 60°C.
  • the sieving, dry pressing, cold isostatic pressing may employ operating conditions known in the art.
  • the sieving is 150-200 mesh sieve.
  • the temperature of the debinding is 250-600°C, preferably 400-550°C, exemplarily 450°C, 500°C, and 550°C.
  • the degumming time is 2-10 hours, preferably 4-8 hours; exemplarily, 2 hours, 4 hours, 6 hours, 8 hours, 10 hours.
  • the powder for embedding does not react with the ceramic green body.
  • the powder for embedding is one or a mixed powder of Al 2 O 3 and Y 2 O 3 .
  • step 3 the powder needs to undergo at least one calcination and crushing treatment before embedding.
  • the powder for embedding before embedding, is calcined and (ground) crushed in air at least once, for example, at least 2 times of calcination and (grinding) crush.
  • the calcination temperature is 1500-1750°C, preferably 1650-1750°C, exemplarily 1500°C, 1600°C, 1650°C, 1700°C, and 1750°C.
  • the calcination time is 4h-15h, preferably 6h-10h, exemplarily 4h, 5h, 6h, 8h, 10h, 12h, 15h.
  • the powder for embedding after at least one calcination and crushing treatment needs to be sieved, for example, 60-150 mesh sieve.
  • the embedding is to uniformly cover the surface of the ceramic green body, preferably the upper and lower surfaces, with the powder for embedding.
  • the thickness of the embedding is 0.3mm-0.6mm, such as 0.4mm-0.5mm.
  • the ceramic green body before vacuum sintering, the ceramic green body is embedded with the treated embedded powder Al 2 O 3 and/or Y 2 O 3 , and the embedded powder is passed through a 60-150 mesh sieve Afterwards, the upper and lower surfaces of the ceramic green body are uniformly covered; preferably, the thickness of the embedded powder covering the upper and lower surfaces of the ceramic green body is 0.3 mm to 0.6 mm, respectively.
  • the vacuum sintering temperature is 1600-1750°C; preferably, the vacuum sintering temperature is 1650-1750°C; more preferably, the vacuum sintering temperature is 1650-1700°C.
  • the holding time of the vacuum sintering is 2 hours to 20 hours, preferably 4 hours to 15 hours; more preferably, 6 hours to 10 hours.
  • the preparation method of the green fluorescent ceramic material includes the following steps:
  • the mixed material is subjected to wet ball milling to obtain a uniformly dispersed slurry
  • the slurry is subjected to vacuum drying, sieving, dry pressing, cold isostatic pressing and degumming procedures to obtain a ceramic green body;
  • the present invention also provides the application of the above-mentioned green fluorescent ceramic material in LED, preferably used as LED packaging material. For example, grinding and polishing the green fluorescent ceramic material to a size required for the LED package, such as 0.1 mm ⁇ 2.0 mm, to obtain a green light transparent ceramic suitable for the LED package.
  • the present invention also provides an LED packaging material, which contains the green fluorescent ceramic material.
  • the present invention also provides an LED device, preferably an LED lighting device, which contains the green fluorescent ceramic material.
  • the green fluorescent ceramic material is a packaging material of an LED device.
  • the light efficiency of the LED device is not lower than 160lm/W, for example, not lower than 165lm/W.
  • the emission peak wavelength of the LED device is in the green light region (490-540 nm).
  • the LED lighting device is an LED green light lighting device; more preferably, an LED green light fish light.
  • the invention overcomes the shortcomings of high equipment requirements in the prior method, reduces the production cost of the graphene-fluorescent ceramic composite material, and obtains a green fluorescent ceramic material with high light efficiency and good heat dissipation.
  • the material is a transparent ceramic material.
  • the introduction of a small amount of graphene through vacuum sintering greatly improves the heat dissipation performance of the green fluorescent ceramic material, and is suitable for packaging materials for high-power LED high-end lighting.
  • Green fluorescent ceramic materials with good heat dissipation are used as packaging materials, which are beneficial to the thermal management of high-power LED lighting and the improvement of service life.
  • FIG. 1 is a transmittance curve diagram of the green light transparent ceramic in Example 1.
  • FIG. 1 is a transmittance curve diagram of the green light transparent ceramic in Example 1.
  • FIG. 2 is an emission spectrum diagram of the green light transparent ceramic in Example 1.
  • FIG. 3 is a physical view of the green light transparent ceramic product in Example 2.
  • FIG. 5 is a physical view of the ceramic product without sintering with buried powder in Comparative Example 4.
  • FIG. 5 is a physical view of the ceramic product without sintering with buried powder in Comparative Example 4.
  • the powder is sieved, dry-pressed, and then pressed into a green body by cold isostatic pressing at 200 MPa.
  • Another Y 2 O 3 powder was repeatedly calcined, ground and crushed twice in the air at 1750°C for 8 h to be used as embedded powder.
  • Y 2 O 3 embedded powder with a thickness of 0.5 mm was spread on the upper and lower surfaces of the green body, and then placed in a vacuum tungsten wire furnace for sintering. The temperature was 1730°C and the sintering time was 4 hours.
  • the ceramic product is ground and polished to 0.8mm to obtain a green light transparent ceramic. Its visible light transmittance reaches 82% (as shown in Figure 1), and the thermal conductivity is 13.2Wm -1 K -1 .
  • the prepared green light transparent ceramics and 150W blue light LED chips were packaged into LED devices. At room temperature, a 2650mA constant current drive is applied, and the performance indicators obtained from the test are as follows:
  • the green light transparent ceramic phosphor in this embodiment has excellent light color quality and thermal conductivity, which is sufficient to meet the requirements for special LED lighting.
  • the prepared green light transparent ceramics were packaged into LED devices, and their properties were tested. Package and test conditions are the same
  • Example 1 The performance indicators obtained from the test are as follows:
  • Fig. 3 is the actual picture of the green light transparent ceramic product in Example 2. It can be seen from Fig. 3 and the above test results that the green light transparent ceramic phosphor in this example has excellent transparency, excellent light color quality and thermal conductivity. , enough to meet the needs of LED special lighting.
  • the prepared green light transparent ceramics were packaged into LED devices, and their properties were tested. Package and test conditions are the same
  • Example 1 The performance indicators obtained from the test are as follows:
  • the green light transparent ceramic phosphor in this embodiment has excellent light color quality and thermal conductivity, which is sufficient to meet the requirements for special LED lighting.
  • Example 1 According to the chemical composition of 0.05wt% graphene-Y 0.0985 Al 5 O 12 : 0.0015Ce 3+ , 2.9Lu 3+ 0.005g graphene, 0.1311g Y 2 O 3 , 3.0047g ⁇ -Al 2 O 3 , 6.7870g Lu 2 O 3 , 0.0030g CeO 2 , 0.005g CaO, 0.05g TEOS raw materials to prepare green transparent ceramics.
  • the difference from Example 1 is that the embedded powder Y 2 O 3 is crushed after being calcined at 1700°C for 10h, and the thickness of the embedded powder is 0.3 mm; °C sintered for 8 hours. Other conditions were the same as those in Example 1, and a green light transparent ceramic material was obtained. The ceramic material was ground and polished to 0.6 mm to obtain a green transparent ceramic. Its visible light transmittance reaches 82%, and its thermal conductivity is 7.2Wm -1 K -1 .
  • the prepared green light transparent ceramics were packaged into LED devices, and their properties were tested. Package and test conditions are the same
  • Example 1 The performance indicators obtained from the test are as follows:
  • the green light transparent ceramic phosphor in this embodiment has excellent light color quality and thermal conductivity, which is sufficient to meet the requirements for special LED lighting.
  • the performance indicators of the packaged LED device are as follows:
  • the performance indicators of the packaged LED device are as follows:
  • Lu 3+ is not doped, its emission wavelength is in the yellow light region, and the light efficiency is lower than that of Example 4 and Comparative Example 1. This can further reflect the superiority of doped Lu 3+ in the present invention for regulating the emission wavelength of the YAG:Ce fluorescent ceramic and enhancing the luminous efficiency.
  • Example 1 The 0.03wt% graphene-Y 2.989 Al 5 O 12 :0.001Ce 3+ ,0.01Lu 3+ green light ceramics in Example 1 were prepared by normal pressure sintering, the difference was that the sintering environment was normal pressure N 2 sintering, and other preparation conditions Same as Example 1. Sintered products have low density and low transparency.
  • the green body is pressureless sintering, and the sintering of ceramic products is hindered by graphene, which reduces the density, which can better reflect the advantages of the vacuum-fired graphene modified green transparent ceramic proposed in the present invention. .
  • Fluorescent ceramics of 0.05wt% graphene-Y 1.495 Al 5 O 12 : 0.003Ce 3+ , 0.5Lu 3+ were prepared according to the procedure in Example 2, the difference was that the ceramics were not embedded in powder before vacuum sintering, and other Preparation conditions are the same as
  • Example 2 The obtained ceramic product has high density and poor transparency, and vacuum sintering forms a large number of oxygen vacancy defects, and the ceramic product is dark brown (as shown in FIG. 5 ). Its luminous intensity is much lower than that of the green ceramic product prepared in Example 2.
  • the LED devices encapsulated in green light ceramics described in the present invention have peak wavelengths in the green light region, high light efficiency, and excellent heat dissipation, which can meet the needs of high-power LED high-end lighting, and also reflect this Excellent properties of green transparent ceramics in the invention.

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  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Structural Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Computer Hardware Design (AREA)
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  • Luminescent Compositions (AREA)

Abstract

Un matériau céramique fluorescent vert, son procédé de préparation et son utilisation, appartenant au domaine des céramiques fluorescentes destinées à l'éclairage par DEL. La constitution chimique du matériau céramique fluorescent vert correspond au graphène-Y 3-x-yAl 5O 12:xCe 3+,yLu 3+, 0,0001 ≤ x ≤ 0,1 et 0,01 ≤ y ≤ 2,9 ; et le pourcentage en masse du graphène étant inférieur à 0,5 % en poids mais n'est pas nul sur la base du poids total du matériau céramique fluorescent vert. Le matériau céramique fluorescent vert a pour caractéristiques une conductivité thermique élevée, une bonne propriété de dissipation de chaleur et une longueur d'onde d'émission de lumière réglable dans une plage comprise de 490 à 540 nm ; et il se prête à une utilisation en tant que matériau d'encapsulation de DEL.
PCT/CN2021/130000 2020-11-11 2021-11-11 Matériau polymère fluorescent vert, son procédé de préparation et son utilisation WO2022100647A1 (fr)

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